Reaktion #2072186

ord-1f3ad7e20b4544669e9e8647b2eea3aa

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe reaction mixture is heated
  2. 2
    Temperaturat reflux
  3. 3
    Sonstigeto return to ambient temperature
  4. 4
    Sonstigethe precipitate obtained
  5. 5
    Filtrationis filtered off
  6. 6
    Waschenwashed with a 35/65 ethanol/water mixture

Vorschrift

173 kg of the compound obtained in Step C and 66 kg of sodium acetate in ethanol are introduced into a 1600 litre reactor. The mixture is stirred and then 79 kg of acetic anhydride are added; the reaction mixture is heated at reflux and 600 l of water are added. The reaction mixture is allowed to return to ambient temperature and the precipitate obtained is filtered off and washed with a 35/65 ethanol/water mixture to give the title product in a yield of 92.5% and with a chemical purity exceeding 99%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07544839B2uspto-grants-2009_06